data_2203345
loop_
_publ_author_name
'Hong Liang'
'Xian-Wen Wang'
'Zhen-Feng Chen'
'Ling Huang'
'Hong-Li Zou'
'Jian Zhou'
'Kai-Bei Yu'
_publ_section_title
;
Aquabis(1,5-dimethyl-2-phenyl-4-{[(E)-4-pyridylmethylene-
\kN]amino}pyrazolidin-3-one)dinitratonickel(II)
;
_journal_issue                 3
_journal_name_full             'Acta Crystallographica, Section E'
_journal_page_first            m294
_journal_page_last             m296
_journal_volume                60
_journal_year                  2004
_chemical_formula_iupac        '[Ni (N O3)2 (C17 H16 N4 O)2 (N O3)2 (H2 O)]'
_chemical_formula_moiety       'C34 H34 N10 Ni O9'
_chemical_formula_sum          'C34 H34 N10 Ni O9'
_chemical_formula_weight       785.42
_chemical_melting_point        ?
_chemical_name_common
;
Dinitratoaquabis(3-pyrazolidinone,
1,5-dimethyl-2-phenyl-4-[{(E)-4-pyridinylmethylidene}amino])nickel(II)
;
_chemical_name_systematic
;
Aquabis(1,5-dimethyl-2-phenyl-4-{[(E)-4-pyridylmethylene-
\kN]amino}pyrazolidin-3-one)dinitratonickel(II)
;
_symmetry_cell_setting         Triclinic
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary   direct
_atom_sites_solution_secondary difmap
_audit_creation_method         SHELXL-97
_cell_angle_alpha              88.860(10)
_cell_angle_beta               75.410(10)
_cell_angle_gamma              73.860(10)
_cell_formula_units_Z          2
_cell_length_a                 10.097(2)
_cell_length_b                 12.977(2)
_cell_length_c                 14.860(2)
_cell_measurement_reflns_used  28
_cell_measurement_temperature  296(2)
_cell_measurement_theta_max    14.59
_cell_measurement_theta_min    2.83
_cell_volume                   1807.3(5)
_computing_cell_refinement     XSCANS
_computing_data_collection     'SXSCANS (Siemens, 1994)'
_computing_data_reduction      'SHELXTL (Sheldrick, 1997a)'
_computing_molecular_graphics  SHELXTL
_computing_publication_material SHELXTL
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution  'SHELXS97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature    296(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method     \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source       'normal-focus sealed tube'
_diffrn_radiation_type         MoK\a
_diffrn_radiation_wavelength   0.71073
_diffrn_reflns_av_R_equivalents 0.0115
_diffrn_reflns_av_sigmaI/netI  0.0402
_diffrn_reflns_limit_h_max     12
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_k_max     15
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_l_max     17
_diffrn_reflns_limit_l_min     -17
_diffrn_reflns_number          7176
_diffrn_reflns_theta_full      25.25
_diffrn_reflns_theta_max       25.25
_diffrn_reflns_theta_min       1.42
_diffrn_standards_decay_%      2.44
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time ?
_diffrn_standards_number       3
_exptl_absorpt_coefficient_mu  0.605
_exptl_absorpt_correction_T_max 0.908
_exptl_absorpt_correction_T_min 0.732
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '(North et al., 1968)'
_exptl_crystal_colour          green
_exptl_crystal_density_diffrn  1.443
_exptl_crystal_density_meas    ?
_exptl_crystal_density_method  'not measured'
_exptl_crystal_description     block
_exptl_crystal_F_000           816
_exptl_crystal_size_max        0.52
_exptl_crystal_size_mid        0.50
_exptl_crystal_size_min        0.16
_refine_diff_density_max       0.415
_refine_diff_density_min       -0.297
_refine_ls_extinction_coef     0.0020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method   SHELXL97
_refine_ls_goodness_of_fit_ref 0.977
_refine_ls_hydrogen_treatment  constr
_refine_ls_matrix_type         full
_refine_ls_number_parameters   500
_refine_ls_number_reflns       6540
_refine_ls_number_restraints   2
_refine_ls_restrained_S_all    0.977
_refine_ls_R_factor_all        0.0540
_refine_ls_R_factor_gt         0.0380
_refine_ls_shift/su_max        0.000
_refine_ls_shift/su_mean       0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0539P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme    calc
_refine_ls_wR_factor_gt        0.0901
_refine_ls_wR_factor_ref       0.0945
_reflns_number_gt              4930
_reflns_number_total           6540
_reflns_threshold_expression   I>2\s(I)
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ni 0.39893(3) 0.21672(2) 0.23919(2) 0.03265(11) Uani d . 1 . . Ni
O1 -0.0322(2) 0.80716(15) 0.61519(12) 0.0559(5) Uani d . 1 . . O
O2 0.9364(2) -0.34901(16) -0.14942(13) 0.0597(5) Uani d . 1 . . O
O3 0.3665(2) 0.18154(15) 0.37970(13) 0.0537(5) Uani d . 1 . . O
O4 0.5556(2) 0.22702(16) 0.32389(16) 0.0683(6) Uani d . 1 . . O
O5 0.4936(3) 0.1973(3) 0.47117(17) 0.1102(10) Uani d . 1 . . O
O6 0.44602(19) 0.26009(15) 0.10393(12) 0.0501(5) Uani d . 1 . . O
O7 0.6117(2) 0.28237(19) -0.00933(15) 0.0837(8) Uani d . 1 . . O
O8 0.6468(3) 0.2606(2) 0.1273(2) 0.0980(9) Uani d . 1 . . O
O9 0.22006(18) 0.18917(14) 0.22241(13) 0.0362(4) Uani d D 1 . . O
N1 0.2993(2) 0.37707(15) 0.28587(13) 0.0355(5) Uani d . 1 . . N
N2 0.2006(2) 0.74980(15) 0.42712(13) 0.0383(5) Uani d . 1 . . N
N3 0.1737(2) 0.98261(15) 0.55898(14) 0.0407(5) Uani d . 1 . . N
N4 0.0635(2) 0.94957(16) 0.61731(13) 0.0411(5) Uani d . 1 . . N
N5 0.5139(2) 0.05842(15) 0.19321(14) 0.0365(5) Uani d . 1 . . N
N6 0.9103(2) -0.27563(16) 0.05646(14) 0.0398(5) Uani d . 1 . . N
N7 1.2171(2) -0.48092(16) -0.05934(14) 0.0432(5) Uani d . 1 . . N
N8 1.1478(2) -0.46009(16) -0.13035(14) 0.0437(5) Uani d . 1 . . N
N9 0.4740(3) 0.20195(18) 0.39484(16) 0.0522(6) Uani d . 1 . . N
N10 0.5725(3) 0.26739(17) 0.07371(16) 0.0480(6) Uani d . 1 . . N
C1 0.1623(3) 0.41141(19) 0.33369(18) 0.0434(6) Uani d . 1 . . C
H1 0.1048 0.3659 0.3364 0.052 Uiso calc R 1 . . H
C2 0.1032(3) 0.5113(2) 0.37892(18) 0.0440(6) Uani d . 1 . . C
H2 0.0072 0.5325 0.4107 0.053 Uiso calc R 1 . . H
C3 0.1867(3) 0.58083(18) 0.37736(16) 0.0370(6) Uani d . 1 . . C
C4 0.3259(3) 0.54678(19) 0.32414(18) 0.0438(6) Uani d . 1 . . C
H4 0.3844 0.5920 0.3177 0.053 Uiso calc R 1 . . H
C5 0.3779(3) 0.44577(19) 0.28055(18) 0.0432(6) Uani d . 1 . . C
H5 0.4724 0.4242 0.2457 0.052 Uiso calc R 1 . . H
C6 0.1303(3) 0.68107(19) 0.43576(17) 0.0403(6) Uani d . 1 . . C
H6 0.0425 0.6944 0.4794 0.048 Uiso calc R 1 . . H
C7 0.0539(3) 0.85678(19) 0.57731(17) 0.0386(6) Uani d . 1 . . C
C8 0.1578(3) 0.83771(18) 0.49016(16) 0.0349(5) Uani d . 1 . . C
C9 0.2268(3) 0.91701(19) 0.48172(17) 0.0380(6) Uani d . 1 . . C
C10 0.3379(3) 0.9348(2) 0.40094(18) 0.0524(7) Uani d . 1 . . C
H10A 0.2965 0.9952 0.3687 0.063 Uiso calc R 1 . . H
H10B 0.3755 0.8719 0.3594 0.063 Uiso calc R 1 . . H
H10C 0.4134 0.9489 0.4225 0.063 Uiso calc R 1 . . H
C11 0.2007(3) 1.0826(2) 0.5768(2) 0.0565(8) Uani d . 1 . . C
H11A 0.2733 1.0950 0.5256 0.068 Uiso calc R 1 . . H
H11B 0.2321 1.0792 0.6329 0.068 Uiso calc R 1 . . H
H11C 0.1146 1.1403 0.5838 0.068 Uiso calc R 1 . . H
C12 0.0115(3) 0.97854(19) 0.71523(16) 0.0366(6) Uani d . 1 . . C
C13 -0.0896(3) 1.0756(2) 0.74506(19) 0.0507(7) Uani d . 1 . . C
H13 -0.1198 1.1240 0.7024 0.061 Uiso calc R 1 . . H
C14 -0.1453(3) 1.0994(3) 0.8397(2) 0.0686(9) Uani d . 1 . . C
H14 -0.2124 1.1650 0.8610 0.082 Uiso calc R 1 . . H
C15 -0.1026(4) 1.0277(4) 0.9023(2) 0.0773(11) Uani d . 1 . . C
H15 -0.1419 1.0441 0.9657 0.093 Uiso calc R 1 . . H
C16 -0.0013(4) 0.9308(3) 0.8717(2) 0.0703(10) Uani d . 1 . . C
H16 0.0279 0.8821 0.9145 0.084 Uiso calc R 1 . . H
C17 0.0566(3) 0.9065(2) 0.7775(2) 0.0501(7) Uani d . 1 . . C
H17 0.1256 0.8418 0.7565 0.060 Uiso calc R 1 . . H
C18 0.4715(3) 0.0029(2) 0.13734(19) 0.0475(7) Uani d . 1 . . C
H18 0.3791 0.0293 0.1307 0.057 Uiso calc R 1 . . H
C19 0.5566(3) -0.0916(2) 0.08868(19) 0.0500(7) Uani d . 1 . . C
H19 0.5214 -0.1271 0.0504 0.060 Uiso calc R 1 . . H
C20 0.6944(3) -0.13333(18) 0.09696(16) 0.0375(6) Uani d . 1 . . C
C21 0.7367(3) -0.0797(2) 0.15899(19) 0.0490(7) Uani d . 1 . . C
H21 0.8262 -0.1070 0.1702 0.059 Uiso calc R 1 . . H
C22 0.6451(3) 0.0147(2) 0.20412(19) 0.0473(7) Uani d . 1 . . C
H22 0.6763 0.0502 0.2447 0.057 Uiso calc R 1 . . H
C23 0.7931(3) -0.22666(19) 0.03797(17) 0.0406(6) Uani d . 1 . . C
H23 0.7697 -0.2501 -0.0132 0.049 Uiso calc R 1 . . H
C24 1.0198(3) -0.38176(19) -0.09916(17) 0.0408(6) Uani d . 1 . . C
C25 1.0120(3) -0.35584(18) -0.00481(17) 0.0361(5) Uani d . 1 . . C
C26 1.1347(3) -0.4184(2) 0.01558(17) 0.0403(6) Uani d . 1 . . C
C27 1.1749(3) -0.4227(2) 0.10564(19) 0.0556(7) Uani d . 1 . . C
H27A 1.1744 -0.4910 0.1315 0.067 Uiso calc R 1 . . H
H27B 1.1075 -0.3664 0.1482 0.067 Uiso calc R 1 . . H
H27C 1.2685 -0.4135 0.0953 0.067 Uiso calc R 1 . . H
C28 1.3593(3) -0.5513(2) -0.0726(2) 0.0578(8) Uani d . 1 . . C
H28A 1.4271 -0.5111 -0.0934 0.069 Uiso calc R 1 . . H
H28B 1.3752 -0.6075 -0.1185 0.069 Uiso calc R 1 . . H
H28C 1.3704 -0.5822 -0.0148 0.069 Uiso calc R 1 . . H
C29 1.2146(3) -0.4958(2) -0.22557(17) 0.0422(6) Uani d . 1 . . C
C30 1.2530(3) -0.4228(2) -0.2882(2) 0.0577(8) Uani d . 1 . . C
H30 1.2394 -0.3524 -0.2678 0.069 Uiso calc R 1 . . H
C31 1.3114(4) -0.4545(3) -0.3809(2) 0.0759(10) Uani d . 1 . . C
H31 1.3369 -0.4053 -0.4232 0.091 Uiso calc R 1 . . H
C32 1.3321(4) -0.5577(3) -0.4110(2) 0.0788(11) Uani d . 1 . . C
H32 1.3709 -0.5786 -0.4738 0.095 Uiso calc R 1 . . H
C33 1.2957(4) -0.6301(3) -0.3489(2) 0.0796(11) Uani d . 1 . . C
H33 1.3120 -0.7009 -0.3694 0.096 Uiso calc R 1 . . H
C34 1.2348(3) -0.5994(2) -0.2556(2) 0.0628(8) Uani d . 1 . . C
H34 1.2077 -0.6487 -0.2138 0.075 Uiso calc R 1 . . H
H9A 0.175(3) 0.232(2) 0.1935(19) 0.069(11) Uiso d D 1 . . H
H9B 0.164(3) 0.177(3) 0.2686(14) 0.074(11) Uiso d D 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni 0.03375(18) 0.02775(17) 0.03507(18) -0.00897(12) -0.00569(13) -0.00348(12)
O1 0.0636(12) 0.0547(11) 0.0489(11) -0.0377(10) 0.0110(9) -0.0155(9)
O2 0.0564(12) 0.0585(12) 0.0496(12) 0.0139(10) -0.0205(10) -0.0068(9)
O3 0.0662(13) 0.0472(11) 0.0540(12) -0.0207(10) -0.0221(10) 0.0090(9)
O4 0.0587(13) 0.0513(12) 0.0859(17) -0.0167(10) -0.0005(12) -0.0082(11)
O5 0.116(2) 0.147(3) 0.0616(16) 0.0057(19) -0.0569(16) -0.0179(16)
O6 0.0426(11) 0.0548(11) 0.0450(11) -0.0131(9) 0.0019(9) 0.0038(9)
O7 0.0737(16) 0.0930(18) 0.0561(14) -0.0145(13) 0.0227(12) 0.0143(12)
O8 0.0881(19) 0.117(2) 0.109(2) -0.0341(17) -0.0552(17) 0.0112(17)
O9 0.0326(10) 0.0356(10) 0.0388(11) -0.0089(8) -0.0067(9) -0.0022(8)
N1 0.0404(12) 0.0288(10) 0.0362(11) -0.0096(9) -0.0075(9) -0.0024(8)
N2 0.0460(12) 0.0298(11) 0.0358(11) -0.0092(9) -0.0062(9) -0.0027(8)
N3 0.0501(13) 0.0304(11) 0.0402(12) -0.0191(10) -0.0004(10) -0.0034(9)
N4 0.0496(13) 0.0378(11) 0.0355(11) -0.0217(10) 0.0009(10) -0.0075(9)
N5 0.0320(11) 0.0345(11) 0.0416(12) -0.0079(9) -0.0080(9) -0.0058(9)
N6 0.0403(12) 0.0318(11) 0.0408(12) -0.0072(9) -0.0016(10) -0.0017(9)
N7 0.0366(12) 0.0429(12) 0.0445(13) -0.0007(10) -0.0123(10) 0.0045(10)
N8 0.0418(12) 0.0402(12) 0.0375(12) 0.0065(10) -0.0091(10) -0.0039(9)
N9 0.0624(16) 0.0463(14) 0.0412(14) -0.0040(12) -0.0129(13) -0.0089(11)
N10 0.0503(14) 0.0398(12) 0.0453(14) -0.0105(11) 0.0010(12) -0.0003(10)
C1 0.0439(15) 0.0362(14) 0.0485(16) -0.0167(12) -0.0020(12) -0.0089(11)
C2 0.0409(15) 0.0397(14) 0.0442(15) -0.0094(12) 0.0007(12) -0.0087(11)
C3 0.0481(15) 0.0272(12) 0.0339(13) -0.0097(11) -0.0080(11) -0.0021(10)
C4 0.0444(15) 0.0331(13) 0.0514(16) -0.0158(12) -0.0016(12) -0.0055(11)
C5 0.0400(14) 0.0343(14) 0.0485(16) -0.0111(11) 0.0019(12) -0.0062(11)
C6 0.0424(14) 0.0329(13) 0.0410(14) -0.0100(11) -0.0026(11) -0.0056(11)
C7 0.0438(14) 0.0335(13) 0.0387(14) -0.0156(11) -0.0055(11) -0.0038(11)
C8 0.0403(14) 0.0266(12) 0.0352(13) -0.0088(10) -0.0054(11) -0.0026(10)
C9 0.0393(14) 0.0340(13) 0.0384(14) -0.0108(11) -0.0056(11) 0.0022(11)
C10 0.0616(18) 0.0466(16) 0.0452(16) -0.0243(14) 0.0038(13) -0.0021(12)
C11 0.073(2) 0.0474(16) 0.0530(17) -0.0343(15) -0.0034(15) -0.0079(13)
C12 0.0406(14) 0.0370(13) 0.0342(13) -0.0162(11) -0.0066(11) -0.0048(10)
C13 0.0510(17) 0.0476(16) 0.0471(16) -0.0056(13) -0.0098(13) -0.0090(13)
C14 0.058(2) 0.075(2) 0.060(2) -0.0089(17) -0.0010(16) -0.0314(18)
C15 0.085(3) 0.119(3) 0.0406(19) -0.058(3) -0.0033(18) -0.015(2)
C16 0.100(3) 0.090(3) 0.051(2) -0.060(2) -0.0364(19) 0.0222(18)
C17 0.0598(18) 0.0434(16) 0.0560(18) -0.0213(14) -0.0231(15) 0.0053(13)
C18 0.0382(15) 0.0430(15) 0.0606(18) -0.0032(12) -0.0190(13) -0.0143(13)
C19 0.0502(16) 0.0426(15) 0.0574(17) -0.0055(13) -0.0212(14) -0.0169(13)
C20 0.0395(14) 0.0312(13) 0.0373(14) -0.0073(11) -0.0050(11) -0.0007(10)
C21 0.0378(14) 0.0419(15) 0.0649(19) -0.0023(12) -0.0174(13) -0.0125(13)
C22 0.0394(15) 0.0435(15) 0.0583(18) -0.0051(12) -0.0172(13) -0.0162(13)
C23 0.0444(15) 0.0336(13) 0.0377(14) -0.0074(12) -0.0033(12) -0.0041(11)
C24 0.0399(14) 0.0338(13) 0.0422(15) -0.0002(11) -0.0099(12) -0.0005(11)
C25 0.0368(13) 0.0295(12) 0.0388(14) -0.0076(11) -0.0055(11) -0.0001(10)
C26 0.0418(14) 0.0391(14) 0.0387(14) -0.0109(12) -0.0087(12) 0.0033(11)
C27 0.0538(18) 0.0651(19) 0.0487(17) -0.0134(15) -0.0184(14) 0.0038(14)
C28 0.0449(16) 0.0506(17) 0.066(2) 0.0073(13) -0.0163(14) -0.0030(14)
C29 0.0369(14) 0.0389(14) 0.0417(15) -0.0020(11) -0.0032(11) -0.0002(11)
C30 0.0590(19) 0.0453(17) 0.0597(19) -0.0100(14) -0.0047(15) 0.0068(14)
C31 0.071(2) 0.086(3) 0.053(2) -0.015(2) 0.0053(17) 0.0190(19)
C32 0.073(2) 0.104(3) 0.0430(19) -0.012(2) 0.0016(17) -0.010(2)
C33 0.092(3) 0.068(2) 0.064(2) -0.022(2) 0.0077(19) -0.0271(18)
C34 0.078(2) 0.0448(17) 0.0531(18) -0.0168(16) 0.0050(16) -0.0058(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O9 Ni O6 . . 89.89(8) ?
O9 Ni N5 . . 90.30(7) ?
O6 Ni N5 . . 88.87(8) ?
O9 Ni N1 . . 94.27(7) ?
O6 Ni N1 . . 90.90(8) ?
N5 Ni N1 . . 175.42(8) yes
O9 Ni O3 . . 96.10(8) ?
O6 Ni O3 . . 173.65(8) ?
N5 Ni O3 . . 93.17(8) ?
N1 Ni O3 . . 86.59(8) ?
O9 Ni O4 . . 153.77(8) ?
O6 Ni O4 . . 116.31(8) ?
N5 Ni O4 . . 91.39(7) ?
N1 Ni O4 . . 84.61(8) ?
O3 Ni O4 . . 57.67(8) yes
N9 O3 Ni . . 98.59(16) ?
N9 O4 Ni . . 89.21(16) ?
N10 O6 Ni . . 114.13(16) ?
Ni O9 H9A . . 116(2) ?
Ni O9 H9B . . 118(2) ?
H9A O9 H9B . . 107(3) ?
C5 N1 C1 . . 117.2(2) ?
C5 N1 Ni . . 119.57(16) ?
C1 N1 Ni . . 122.46(16) ?
C6 N2 C8 . . 120.7(2) ?
C9 N3 N4 . . 108.51(18) ?
C9 N3 C11 . . 128.7(2) ?
N4 N3 C11 . . 121.9(2) ?
C7 N4 N3 . . 108.75(18) ?
C7 N4 C12 . . 123.34(19) ?
N3 N4 C12 . . 123.45(19) ?
C18 N5 C22 . . 116.0(2) ?
C18 N5 Ni . . 121.16(17) ?
C22 N5 Ni . . 121.83(16) ?
C23 N6 C25 . . 120.8(2) ?
C26 N7 N8 . . 108.23(19) ?
C26 N7 C28 . . 128.6(2) ?
N8 N7 C28 . . 122.9(2) ?
C24 N8 N7 . . 109.4(2) ?
C24 N8 C29 . . 125.2(2) ?
N7 N8 C29 . . 123.9(2) ?
O5 N9 O3 . . 121.0(3) ?
O5 N9 O4 . . 124.6(3) ?
O3 N9 O4 . . 114.4(2) ?
O8 N10 O7 . . 123.6(3) ?
O8 N10 O6 . . 119.3(2) ?
O7 N10 O6 . . 117.1(3) ?
N1 C1 C2 . . 122.6(2) ?
N1 C1 H1 . . 118.7 ?
C2 C1 H1 . . 118.7 ?
C1 C2 C3 . . 120.2(2) ?
C1 C2 H2 . . 119.9 ?
C3 C2 H2 . . 119.9 ?
C4 C3 C2 . . 116.7(2) ?
C4 C3 C6 . . 122.6(2) ?
C2 C3 C6 . . 120.5(2) ?
C5 C4 C3 . . 119.9(2) ?
C5 C4 H4 . . 120.1 ?
C3 C4 H4 . . 120.1 ?
N1 C5 C4 . . 123.2(2) ?
N1 C5 H5 . . 118.4 ?
C4 C5 H5 . . 118.4 ?
N2 C6 C3 . . 120.4(2) ?
N2 C6 H6 . . 119.8 ?
C3 C6 H6 . . 119.8 ?
O1 C7 N4 . . 123.2(2) ?
O1 C7 C8 . . 131.3(2) ?
N4 C7 C8 . . 105.54(19) ?
C9 C8 N2 . . 123.0(2) ?
C9 C8 C7 . . 107.9(2) ?
N2 C8 C7 . . 128.6(2) ?
N3 C9 C8 . . 109.2(2) ?
N3 C9 C10 . . 122.8(2) ?
C8 C9 C10 . . 128.0(2) ?
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
N3 C11 H11A . . 109.5 ?
N3 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
N3 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C17 C12 C13 . . 121.2(2) ?
C17 C12 N4 . . 119.4(2) ?
C13 C12 N4 . . 119.3(2) ?
C12 C13 C14 . . 118.7(3) ?
C12 C13 H13 . . 120.7 ?
C14 C13 H13 . . 120.7 ?
C15 C14 C13 . . 120.6(3) ?
C15 C14 H14 . . 119.7 ?
C13 C14 H14 . . 119.7 ?
C14 C15 C16 . . 120.3(3) ?
C14 C15 H15 . . 119.9 ?
C16 C15 H15 . . 119.9 ?
C17 C16 C15 . . 119.8(3) ?
C17 C16 H16 . . 120.1 ?
C15 C16 H16 . . 120.1 ?
C12 C17 C16 . . 119.5(3) ?
C12 C17 H17 . . 120.2 ?
C16 C17 H17 . . 120.2 ?
N5 C18 C19 . . 123.8(2) ?
N5 C18 H18 . . 118.1 ?
C19 C18 H18 . . 118.1 ?
C18 C19 C20 . . 119.8(2) ?
C18 C19 H19 . . 120.1 ?
C20 C19 H19 . . 120.1 ?
C21 C20 C19 . . 116.9(2) ?
C21 C20 C23 . . 122.0(2) ?
C19 C20 C23 . . 121.0(2) ?
C22 C21 C20 . . 119.3(2) ?
C22 C21 H21 . . 120.3 ?
C20 C21 H21 . . 120.3 ?
N5 C22 C21 . . 124.1(2) ?
N5 C22 H22 . . 117.9 ?
C21 C22 H22 . . 117.9 ?
N6 C23 C20 . . 120.4(2) ?
N6 C23 H23 . . 119.8 ?
C20 C23 H23 . . 119.8 ?
O2 C24 N8 . . 122.2(2) ?
O2 C24 C25 . . 132.5(2) ?
N8 C24 C25 . . 105.2(2) ?
C26 C25 N6 . . 123.2(2) ?
C26 C25 C24 . . 107.7(2) ?
N6 C25 C24 . . 128.8(2) ?
N7 C26 C25 . . 109.4(2) ?
N7 C26 C27 . . 122.4(2) ?
C25 C26 C27 . . 128.1(2) ?
C26 C27 H27A . . 109.5 ?
C26 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
C26 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
N7 C28 H28A . . 109.5 ?
N7 C28 H28B . . 109.5 ?
H28A C28 H28B . . 109.5 ?
N7 C28 H28C . . 109.5 ?
H28A C28 H28C . . 109.5 ?
H28B C28 H28C . . 109.5 ?
C34 C29 C30 . . 120.1(3) ?
C34 C29 N8 . . 121.0(2) ?
C30 C29 N8 . . 118.8(2) ?
C31 C30 C29 . . 119.7(3) ?
C31 C30 H30 . . 120.2 ?
C29 C30 H30 . . 120.2 ?
C32 C31 C30 . . 120.4(3) ?
C32 C31 H31 . . 119.8 ?
C30 C31 H31 . . 119.8 ?
C33 C32 C31 . . 119.9(3) ?
C33 C32 H32 . . 120.1 ?
C31 C32 H32 . . 120.1 ?
C32 C33 C34 . . 120.7(3) ?
C32 C33 H33 . . 119.7 ?
C34 C33 H33 . . 119.7 ?
C29 C34 C33 . . 119.3(3) ?
C29 C34 H34 . . 120.3 ?
C33 C34 H34 . . 120.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni O9 . 2.0104(18) yes
Ni O6 . 2.0506(18) yes
Ni N5 . 2.0892(19) yes
Ni N1 . 2.0892(19) yes
Ni O3 . 2.0920(19) yes
Ni O4 . 2.287(2) yes
O1 C7 . 1.240(3) yes
O2 C24 . 1.247(3) yes
O3 N9 . 1.258(3) ?
O4 N9 . 1.263(3) ?
O5 N9 . 1.197(3) ?
O6 N10 . 1.272(3) ?
O7 N10 . 1.227(3) ?
O8 N10 . 1.212(3) ?
O9 H9A . 0.811(10) ?
O9 H9B . 0.817(10) ?
N1 C5 . 1.338(3) ?
N1 C1 . 1.339(3) ?
N2 C6 . 1.272(3) yes
N2 C8 . 1.389(3) ?
N3 C9 . 1.344(3) ?
N3 N4 . 1.392(3) ?
N3 C11 . 1.441(3) ?
N4 C7 . 1.391(3) ?
N4 C12 . 1.436(3) ?
N5 C18 . 1.329(3) ?
N5 C22 . 1.338(3) ?
N6 C23 . 1.273(3) yes
N6 C25 . 1.392(3) ?
N7 C26 . 1.335(3) ?
N7 N8 . 1.390(3) ?
N7 C28 . 1.439(3) ?
N8 C24 . 1.380(3) ?
N8 C29 . 1.430(3) ?
C1 C2 . 1.375(3) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.392(3) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.380(3) ?
C3 C6 . 1.468(3) ?
C4 C5 . 1.376(3) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.422(3) ?
C8 C9 . 1.382(3) ?
C9 C10 . 1.485(3) ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 C17 . 1.371(3) ?
C12 C13 . 1.380(3) ?
C13 C14 . 1.383(4) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.364(5) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.381(5) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.379(4) ?
C16 H16 . 0.9300 ?
C17 H17 . 0.9300 ?
C18 C19 . 1.379(3) ?
C18 H18 . 0.9300 ?
C19 C20 . 1.382(4) ?
C19 H19 . 0.9300 ?
C20 C21 . 1.380(3) ?
C20 C23 . 1.469(3) ?
C21 C22 . 1.377(3) ?
C21 H21 . 0.9300 ?
C22 H22 . 0.9300 ?
C23 H23 . 0.9300 ?
C24 C25 . 1.426(3) ?
C25 C26 . 1.381(3) ?
C26 C27 . 1.489(4) ?
C27 H27A . 0.9600 ?
C27 H27B . 0.9600 ?
C27 H27C . 0.9600 ?
C28 H28A . 0.9600 ?
C28 H28B . 0.9600 ?
C28 H28C . 0.9600 ?
C29 C34 . 1.369(4) ?
C29 C30 . 1.379(4) ?
C30 C31 . 1.376(4) ?
C30 H30 . 0.9300 ?
C31 C32 . 1.363(5) ?
C31 H31 . 0.9300 ?
C32 C33 . 1.362(5) ?
C32 H32 . 0.9300 ?
C33 C34 . 1.384(4) ?
C33 H33 . 0.9300 ?
C34 H34 . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O9 H9A O2 . . 2_655 0.81 1.84 2.632(3) 168 yes
O9 H9B O1 . . 2_566 0.82 1.87 2.659(3) 162 yes
C10 H10C O5 . . 2_666 0.94 2.57 3.053(4) 111 yes
C11 H11A O3 . . 1_565 0.96 2.51 3.407(4) 155 yes
C14 H14 O7 . . 1_466 0.93 2.46 3.300(4) 149 yes
C27 H27C O7 . . 2_755 0.96 2.50 3.245(4) 134 yes
C28 H28C O7 . . 1_645 0.96 2.60 3.179(4) 119 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O9 Ni O3 N9 . . . . -177.49(15) ?
N5 Ni O3 N9 . . . . 91.87(15) ?
N1 Ni O3 N9 . . . . -83.55(15) ?
O4 Ni O3 N9 . . . . 2.22(13) ?
O9 Ni O4 N9 . . . . -1.5(2) ?
O6 Ni O4 N9 . . . . 175.51(13) ?
N5 Ni O4 N9 . . . . -95.06(15) ?
N1 Ni O4 N9 . . . . 87.18(15) ?
O3 Ni O4 N9 . . . . -2.19(13) ?
O9 Ni O6 N10 . . . . -167.43(16) ?
N5 Ni O6 N10 . . . . -77.13(17) ?
N1 Ni O6 N10 . . . . 98.30(17) ?
O4 Ni O6 N10 . . . . 13.87(19) ?
O9 Ni N1 C5 . . . . -159.00(19) ?
O6 Ni N1 C5 . . . . -69.05(19) ?
O3 Ni N1 C5 . . . . 105.12(19) ?
O4 Ni N1 C5 . . . . 47.30(19) ?
O9 Ni N1 C1 . . . . 31.1(2) ?
O6 Ni N1 C1 . . . . 121.0(2) ?
O3 Ni N1 C1 . . . . -64.8(2) ?
O4 Ni N1 C1 . . . . -122.6(2) ?
C9 N3 N4 C7 . . . . 3.6(3) ?
C11 N3 N4 C7 . . . . 173.6(2) ?
C9 N3 N4 C12 . . . . 160.5(2) ?
C11 N3 N4 C12 . . . . -29.5(4) ?
O9 Ni N5 C18 . . . . 25.5(2) ?
O6 Ni N5 C18 . . . . -64.4(2) ?
O3 Ni N5 C18 . . . . 121.6(2) ?
O4 Ni N5 C18 . . . . 179.3(2) ?
O9 Ni N5 C22 . . . . -166.8(2) ?
O6 Ni N5 C22 . . . . 103.4(2) ?
O3 Ni N5 C22 . . . . -70.6(2) ?
O4 Ni N5 C22 . . . . -12.9(2) ?
C26 N7 N8 C24 . . . . 0.7(3) ?
C28 N7 N8 C24 . . . . -173.9(2) ?
C26 N7 N8 C29 . . . . 167.2(2) ?
C28 N7 N8 C29 . . . . -7.3(4) ?
Ni O3 N9 O5 . . . . 176.1(2) ?
Ni O3 N9 O4 . . . . -3.7(2) ?
Ni O4 N9 O5 . . . . -176.5(3) ?
Ni O4 N9 O3 . . . . 3.4(2) ?
Ni O6 N10 O8 . . . . -8.0(3) ?
Ni O6 N10 O7 . . . . 172.83(18) ?
C5 N1 C1 C2 . . . . -2.3(4) ?
Ni N1 C1 C2 . . . . 167.9(2) ?
N1 C1 C2 C3 . . . . -0.9(4) ?
C1 C2 C3 C4 . . . . 3.9(4) ?
C1 C2 C3 C6 . . . . -171.5(2) ?
C2 C3 C4 C5 . . . . -3.9(4) ?
C6 C3 C4 C5 . . . . 171.5(2) ?
C1 N1 C5 C4 . . . . 2.3(4) ?
Ni N1 C5 C4 . . . . -168.1(2) ?
C3 C4 C5 N1 . . . . 0.8(4) ?
C8 N2 C6 C3 . . . . -171.2(2) ?
C4 C3 C6 N2 . . . . 12.3(4) ?
C2 C3 C6 N2 . . . . -172.5(2) ?
N3 N4 C7 O1 . . . . 177.7(2) ?
C12 N4 C7 O1 . . . . 20.8(4) ?
N3 N4 C7 C8 . . . . -2.8(3) ?
C12 N4 C7 C8 . . . . -159.8(2) ?
C6 N2 C8 C9 . . . . -177.2(2) ?
C6 N2 C8 C7 . . . . 11.7(4) ?
O1 C7 C8 C9 . . . . -179.5(3) ?
N4 C7 C8 C9 . . . . 1.1(3) ?
O1 C7 C8 N2 . . . . -7.3(5) ?
N4 C7 C8 N2 . . . . 173.3(2) ?
N4 N3 C9 C8 . . . . -2.9(3) ?
C11 N3 C9 C8 . . . . -172.0(3) ?
N4 N3 C9 C10 . . . . 174.7(2) ?
C11 N3 C9 C10 . . . . 5.6(4) ?
N2 C8 C9 N3 . . . . -171.6(2) ?
C7 C8 C9 N3 . . . . 1.1(3) ?
N2 C8 C9 C10 . . . . 11.0(4) ?
C7 C8 C9 C10 . . . . -176.3(3) ?
C7 N4 C12 C17 . . . . 54.0(3) ?
N3 N4 C12 C17 . . . . -99.6(3) ?
C7 N4 C12 C13 . . . . -121.9(3) ?
N3 N4 C12 C13 . . . . 84.5(3) ?
C17 C12 C13 C14 . . . . 0.1(4) ?
N4 C12 C13 C14 . . . . 176.0(2) ?
C12 C13 C14 C15 . . . . -1.0(5) ?
C13 C14 C15 C16 . . . . 1.1(5) ?
C14 C15 C16 C17 . . . . -0.2(5) ?
C13 C12 C17 C16 . . . . 0.8(4) ?
N4 C12 C17 C16 . . . . -175.1(2) ?
C15 C16 C17 C12 . . . . -0.7(4) ?
C22 N5 C18 C19 . . . . -3.1(4) ?
Ni N5 C18 C19 . . . . 165.3(2) ?
N5 C18 C19 C20 . . . . 0.1(4) ?
C18 C19 C20 C21 . . . . 3.6(4) ?
C18 C19 C20 C23 . . . . -172.8(2) ?
C19 C20 C21 C22 . . . . -4.2(4) ?
C23 C20 C21 C22 . . . . 172.2(2) ?
C18 N5 C22 C21 . . . . 2.5(4) ?
Ni N5 C22 C21 . . . . -165.9(2) ?
C20 C21 C22 N5 . . . . 1.2(4) ?
C25 N6 C23 C20 . . . . -172.3(2) ?
C21 C20 C23 N6 . . . . 15.8(4) ?
C19 C20 C23 N6 . . . . -168.0(2) ?
N7 N8 C24 O2 . . . . -179.4(2) ?
C29 N8 C24 O2 . . . . 14.3(4) ?
N7 N8 C24 C25 . . . . -0.7(3) ?
C29 N8 C24 C25 . . . . -167.1(2) ?
C23 N6 C25 C26 . . . . -173.7(2) ?
C23 N6 C25 C24 . . . . 13.5(4) ?
O2 C24 C25 C26 . . . . 179.0(3) ?
N8 C24 C25 C26 . . . . 0.5(3) ?
O2 C24 C25 N6 . . . . -7.3(5) ?
N8 C24 C25 N6 . . . . 174.3(2) ?
N8 N7 C26 C25 . . . . -0.3(3) ?
C28 N7 C26 C25 . . . . 173.8(3) ?
N8 N7 C26 C27 . . . . 178.0(2) ?
C28 N7 C26 C27 . . . . -7.8(4) ?
N6 C25 C26 N7 . . . . -174.3(2) ?
C24 C25 C26 N7 . . . . -0.1(3) ?
N6 C25 C26 C27 . . . . 7.5(4) ?
C24 C25 C26 C27 . . . . -178.4(3) ?
C24 N8 C29 C34 . . . . -116.4(3) ?
N7 N8 C29 C34 . . . . 79.2(4) ?
C24 N8 C29 C30 . . . . 60.7(4) ?
N7 N8 C29 C30 . . . . -103.8(3) ?
C34 C29 C30 C31 . . . . 0.1(5) ?
N8 C29 C30 C31 . . . . -177.0(3) ?
C29 C30 C31 C32 . . . . -0.3(5) ?
C30 C31 C32 C33 . . . . -0.5(6) ?
C31 C32 C33 C34 . . . . 1.5(6) ?
C30 C29 C34 C33 . . . . 0.9(5) ?
N8 C29 C34 C33 . . . . 177.9(3) ?
C32 C33 C34 C29 . . . . -1.7(6) ?